CN101182602A - Tantalum and/or powder for powder metallurgy and method of producing the same - Google Patents
Tantalum and/or powder for powder metallurgy and method of producing the same Download PDFInfo
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Abstract
The invention relates to a tantalum and/or niobium powder for powder metallurgy; the oxygen content of the tantalum and/or niobium powder is not higher than 1500ppjm and the nitrogen content is not higher than 200ppm; the specific surface area of the tantalum powder is not more than 0.15m2/g and the apparent density is between 3.5 to 7.0g/cm3. The production steps comprise that the raw materials of tantalum and/or niobium powders are compressed into strips; the compressed strips are sintered in vacuum; the sintered strips are hydrogenated into powder; the hydrogenated tantalum and/or niobium powders are dried and added with reducing metal for thermal treatments of oxidization and dehydrogenation; the tantalum and/or niobium powders after the thermal treatment are washed by acid and water and dried.
Description
Technical field:
The invention belongs to the rare metal field of smelting, relate to tantalum and niobium powder processing technology, particularly a kind of powder used in metallurgy tantalum and/or niobium powder and preparation method thereof.
Background technology:
Tantalum, niobium are the elements of similar performance, because their fusing point height (fusing point of tantalum is 2996 ℃, and the fusing point of niobium is 2468 ℃), steam force down, good, the anti-liquid metal corrosion of cold-forming property and the strong acid corrosive power except that hydrofluoric acid is strong, chemical stability is high, the dielectricity of its oxide film is good.Thereby tantalum, niobium be processed to various materials such as rod, plate, sheet, pipe, silk, paper tinsel, is widely used in making heat generating components, charging tray and the heat preservation component in electrolytic capacitor anode, the vacuum high temperature furnace, the impregnating material of chemical industry equipment and the sputtering target material that is used for the blocking layer between integrated circuit interconnection copper cash and the silicon.The usage quantity maximum be to make electrolytic condenser, tantalum, niobium powder and tantalum wire, niobium silk be as capacitor anode, tantalum piece, niobium sheet are used for deep-draw and are processed into capacitor case.
That the working method of tantalum, niobium processing material has is rolling behind the melting ingot casting, drawing method for processing and the rolling drawing method for processing of powder metallurgy.The former carries out sintering to tantalum and/or niobium powder compacting slivering, and electron beam melting and/or arc melting are processed then then; The latter is with High-purity Tantalum and/or niobium powder compression moulding, processes behind the sintering.A kind of method operational path in back is short, the lumber recovery height, and it is thin and texture uniform processing material has the better processability energy, the product longer service life that obtains to be more convenient for obtaining crystal grain.
Different purposes according to tantalum, niobium powder have different requirements to its chemical purity and physical property.As the raw material of powder metallurgy, as tantalum and/or niobium powder, must have high purity, expectation interstitial element content is low, so that the blank that obtains has good ductility, for example the tantalum powder is expected oxygen level below 1500ppm, nitrogen content is below 200ppm.The niobium powder wishes that also similar impurity content is arranged.
Usually use sodium Metal 99.5 to also have tantalum potassium fluoride or potassium niobate fluoride to produce tantalum, niobium powder, this powder that obtains is the porous aggregated particle, and its specific surface area is big, and loose density is little, and sodium reduction tantalum powder loose density is usually less than 3.5g/cm
3(density of 20 ℃ of tantalums is 16.64g/cm
3), the loose density of sodium reduction niobium powder is usually less than 1.8g/cm
3(density of 20 ℃ of niobiums is 8.66g/cm
3); Corresponding oxygen level is also higher.
And, also to reach certain requirement as the tantalum of the raw material of powder metallurgy and/or some physical property of niobium powder, because tantalum and/or niobium are reactive metals, at normal temperatures with reactions such as O, N, generate the compound of tantalum and/or niobium or be solidly soluted in the matrix, so the O of tantalum and/or niobium powder, N content and specific surface area have direct relation, specific surface area is big more, and O, N content are high more.Because tantalum and/or niobium powder form fine and close oxide film at particle surface, its specific surface area is directly proportional so the tantalum after the deoxidation and/or the oxygen level of niobium powder are made peace greatly, so tantalum and/or niobium powder as powder used in metallurgy expect to have less specific surface area, for example, the BET specific surface area of tantalum powder (abbreviation specific surface area) is desirably in 0.15m
2Below/the g, loose density requires greater than 3.5g/cm
3, preferably at 3.5～6.0g/cm
3If the loose density of tantalum powder is less than 3.5g/cm
3, the pressed compact porosity is too big, and the base rod density is big inadequately, can occur disconnected bar during the incipient fusion sintering.The niobium powder also has similar situation.In a word, if tantalum and/or niobium powder big with specific surface area, that oxygen level is high, loose density is little are pressed into larger-size when sintering, because a large amount of volatilizations of impurity are broken bar, perhaps also not fully volatilization of the impurity at center before the closure of sintered bar surface pore, occur " evil mind ", the sintering blank is difficult to be purified to desired degree of purity, the forging of such sintering blank, calenderability is poor, will ftracture in rolling processing.
In the prior art, as US 4483819, the clear 61-284501 of CN 1052070 and Te Kai discloses the method that reduces oxygen level and groupization valve metal powder in the valve metal powder, and these technology are effective for the capacitor level valve metal powder of manufacturing high-specific surface area.Owing to when contacting, will form new oxide film with oxygen with oxygen-containing medium at tantalum after the high temperature deoxidation and/or niobium powder, thereby the big tantalum of specific surface area and/or niobium powder oxygen level are difficult to be reduced to and are lower than 1500ppm, tantalum and/or niobium powder as powder used in metallurgy, must reduce the specific surface area of tantalum and/or niobium metal powders significantly, and carry out deoxidation treatment.
Foreign matter content height, specific surface area is big, loose density is little tantalum and/or niobium metal powders adopt plasma melting usually or carry out refining through the method for press strip, sintering, arc melting, electron beam melting hydrogenation powder process again, dehydrogenation, but these methods all have the equipment complexity, operational path is long, the problem that the valve metal powder rate of recovery is low, thereby, cost is increased.
Summary of the invention: the objective of the invention is to overcome the prior art defective, a kind of powder used in metallurgy tantalum and/or niobium powder are provided; Another object of the present invention provides the preparation method of powder used in metallurgy tantalum and/or niobium powder.
Purpose of the present invention realizes by following scheme: a kind of powder used in metallurgy tantalum and/or niobium powder, and the oxygen level of tantalum powder and/or niobium powder is not higher than 1500ppm, and nitrogen content is not higher than 200ppm, and the specific surface area of tantalum powder is not more than 0.15m
2/ g, loose density is at 3.5～7.0g/cm
3In the scope, niobium powder specific surface area is not more than 0.30m
2/ g, loose density is at 2.0～4.0g/cm
3In the scope.
The production stage of described powder used in metallurgy tantalum and/or niobium powder comprises: (1) is pressed into the base bar to raw material tantalum and/or niobium powder raw material; (2) the base bar of vacuum sintering compacting; (3) with sintered blank bar hydrogenation powder process; (4) hydrogenant tantalum and/or niobium powder adding reducing metal are carried out deoxidation, dehydrogenation thermal treatment; (5) tantalum after the thermal treatment and/or niobium powder are carried out pickling, washing, oven dry.
The oxygen level of tantalum of the present invention and/or niobium powder through LECO-RO416R apparatus for determination of oxygen pulse heating inertia fusion infrared absorption determining less than 1500ppm, minimum reaching below the 500ppm; BET specific surface area, loose density, Fei Shi median size and D
50Data measure according to the method that the inventor's Chinese patent CN1410209A is narrated, the specific surface area of tantalum powder is not more than 0.15m
2/ g, loose density is at 3.5～7.0g/cm
3In the scope, niobium powder specific surface area is not more than 0.30m
2/ g, loose density is at 2.0～4.0g/cm
3In the scope, satisfy the requirement of powder metallurgy fully; Preparation method of the present invention is simple, practical, and the equipment used investment is little, easy to operate.
Embodiment:
Embodiment 1
Foreign matter contents such as the oxygen of raw material 1 tantalum powder, nitrogen, carbon see Table 1-1; Its specific surface area, loose density, Fei Shi median size and middle diameter see Table 1-2.Above-mentioned tantalum powder is added the silica flour of 1.0% quality, and with forming press above-mentioned raw materials tantalum powder mixture being pressed into density behind the mixing is 6.2g/cm
3Cross section be quadrate tantalum base bar, with described tantalum briquet 1.33Pa with the vacuum oven of overdraft in induction heating to 1750 ℃ kept 4 hours, be cooled to 800 ℃ and feed hydrogen, hydrogen pressure be about 10kPa～30kPa, lowers the temperature to make the hydrogenation of tantalum briquet suction hydrogen.Tantalum briquet after the hydrogenation is by powder crushing process, make tantalum powder footpath less than 140 μ m, the magnesium chips of this pulverized hydrogenated tantal powder with hydrogenated tantal grain weight amount 1.0% quality mixed, and applying argon gas is heated to 850 ℃ in vacuum oven then, is incubated 3 hours, cooling is come out of the stove then, remove unnecessary magnesium and magnesium oxide with the salt acid elution, wash neutrality with deionized water then, the tantalum powder is dried, the refining tantalum powder 1 that obtains detects foreign matter contents such as its oxygen, nitrogen, carbon as table 1-1; Loose density, specific surface area, Fei Shi median size and the middle diameter of refining tantalum powder 1 see Table 1-2.
Table 1-1 raw material 1 tantalum powder and refining tantalum powder 1 impurity atom (ppm)
| O | C | N | H | K | Na | Si | |
| Ta powder 1 | 3800 | 55 | 320 | 120 | 15 | 3 | 15 |
| Refining tantalum powder 1 | 620 | ＜10 | 120 | 30 | 3 | 1 | 520 |
Table 1-2 raw material 1 tantalum powder and embodiment 1 tantalum powder physical property
| Specific surface area cm 2/g | Loose density g/cm 3 | Fei Shi median size μ m | D 50 μm | |
| Ta powder 1 | 8600 | 1.85 | 2.85 | 94.21 |
| Refining tantalum powder 1 | 625 | 4.7 | 9.5 | 75.68 |
Embodiment 2
Foreign matter contents such as the oxygen of Ta powder, nitrogen, carbon see Table 2-1; Its specific surface area, loose density, Fei Shi median size and middle diameter see Table 2-2.Carry out the base bar that isostatic pressing is the circle of diameter 43mm ~ 58mm with raw material 2 tantalum powder, the pressed density of base bar is about 8.5～9.5g/cm
3Above-mentioned tantalum base is heated to 1440 ℃ of insulations carried out sintering in 5 hours in the vacuum oven of 1.33Pa with overdraft, come out of the stove after the cooling and obtain sintered bar, then above-mentioned sintered bar is heated to 800 ℃ of coolings carries out hydrogen treatment, the powder process of tantalum after hydrogenation rod is obtained the hydrogenated tantal powder of particle diameter less than 140 μ m, in the hydrogenated tantal powder, sneak into 1% magnesium chips, in argon gas atmosphere in the airtight stove, be heated to 850 ℃ of insulations and carried out dehydrogenation in 3 hours, deoxidation treatment, cooled tantalum pruinescence takes out and carries out pickling, with washing neutrality with deionized water behind the salt acid elution, oven dry obtains the tantalum powder then.This tantalum powder was heat-treated 1 hour at 1450 ℃, and the main impurity atom content of the tantalum powder that obtains is listed among the table 2-1, and the specific surface area of tantalum powder, loose density, Fei Shi median size and middle diameter are listed among the table 2-2.
Table 2-1 raw material 2 tantalum powder and embodiment 2 tantalum efflorescence impurity (ppm)
| 0 | C | N | H | K | Na | |
| Ta powder 2 | 3200 | 25 | 280 | 130 | 10 | 3 |
| Refining tantalum powder 2 | 1100 | 11 | 150 | 20 | 3 | 2 |
Table 2-2 raw material 2 tantalum powder and embodiment 2 tantalum powder physical propertys
| Specific surface area cm 2/g | Loose density 3 g/cm 3 | Fei Shi median size μ m | D 50 μm | |
| Ta powder 2 | 6500 | 1.85 | 2.85 | 90.12 |
| Refining tantalum powder 2 | 1250 | 4.2 | 9.5 | 72.45 |
Embodiment 3
Foreign matter contents such as the oxygen of raw material niobium powder, nitrogen, carbon see Table 3-1; Its specific surface area, loose density, Fei Shi median size and middle diameter see Table 3-2.Carrying out isostatic pressing with raw material 3 niobium powder is that cross-sectional diameter is the base bar of the circle of 40mm ~ 50mm, and the pressed density of base bar is about 5.0～6.0g/cm
3Above-mentioned niobium base is heated to 1240 ℃ of insulations carried out sintering in 4 hours in the vacuum oven of 1.33Pa with overdraft, come out of the stove after the cooling and obtain sintered bar, then above-mentioned sintered bar is heated to 700 ℃ of coolings carries out hydrogen treatment, niobium rod powder process after the hydrogenation obtains the hydrogenated niobium powder of particle diameter less than 140 μ m, in the hydrogenated niobium powder, sneak into 1.2% magnesium chips, in argon gas atmosphere in the airtight stove, be heated to 800 ℃ of insulations and carried out dehydrogenation in 3 hours, deoxidation treatment, cooled niobium pruinescence takes out and carries out pickling, with washing neutrality with deionized water behind the salt acid elution, oven dry obtains the niobium powder then.This niobium powder was heat-treated 1 hour at 1250 ℃, and the main impurity atom content of the niobium powder that obtains is listed among the table 3-1; The specific surface area of niobium powder, loose density, Fei Shi median size and middle diameter are listed among the table 3-2.
Table 3-1 raw material niobium powder 3 and embodiment 3 niobium efflorescence impurity (ppm)
| O | C | N | H | K | Na | |
| Raw material niobium powder 3 | 3600 | 40 | 400 | 150 | 12 | 3 |
| Refining niobium powder 3 | 1200 | 22 | 130 | 20 | 5 | 2 |
Table 3-2 raw material niobium powder 3 and embodiment 3 niobium powder physical propertys
| Specific surface area cm 2/g | Loose density g/cm 3 | Fei Shi median size μ m | D 50 μm | |
| Raw material niobium powder 3 | 8300 | 1.50 | 1.45 | 86.45 |
| Refining niobium powder 3 | 950 | 2.6 | 5.5 | 71.23 |
Embodiment 4
The major impurity content of Ta powder is as shown in table 4-1, and the specific surface area of tantalum powder, loose density, Fei Shi median size and middle diameter see Table 4-2.In above-mentioned tantalum powder, sneak into the yttrium powder of 100ppm, the tantalum powder mixture is carried out isostatic pressing, be pressed into density and be about 9.5～11.0g/cm
3Cross-sectional diameter be the pole tantalum base of 50mm～55mm, with above-mentioned tantalum base 1.33Pa with the vacuum sintering stove of overdraft in resistive heating to 1800 ℃ insulation 2 hours, be warmed up to 2050 ℃ of insulations 4 hours, come out of the stove after the cooling and obtain sintered bar, then above-mentioned sintered bar is heated to 800 ℃ of coolings carries out hydrogen treatment, tantalum rod powder process after the hydrogenation obtains the hydrogenated tantal powder of particle diameter less than 140 μ m, in the hydrogenated tantal powder, sneak into the magnesium chips of 0.6% quality, in argon gas atmosphere in the airtight stove, be heated to 850 ℃ of insulations and carried out dehydrogenation in 3 hours, deoxidation treatment, cooled tantalum pruinescence takes out and carries out pickling, with washing neutrality with deionized water behind the salt acid elution, oven dry obtains the tantalum powder then.The main impurity atom content of tantalum powder is listed among the table 4-1, and the specific surface area of tantalum powder, loose density and Fei Shi median size and middle diameter are listed among the table 4-2.
Table 4-1 Ta powder 4 and embodiment 4 tantalum efflorescence impurity (ppm)
| 0 | C | N | H | K | Na | Y | |
| Ta powder 4 | 2800 | 25 | 230 | 120 | 6 | 3 | - |
| Refining tantalum powder 4 | 310 | ＜10 | 20 | 20 | 3 | 1 | 90 |
Table 4-2 raw material 4 powder and embodiment 4 tantalum powder physical propertys
| Specific surface area cm 2/g | Loose density g/cm 3 | Fei Shi median size μ m | D 50 μm | |
| Ta powder 4 | 5030 | 1.85 | 2.85 | 90.12 |
| Refining tantalum powder 4 | 536 | 5.0 | 12.2 | 81.05 |
From above-mentioned explanation and embodiment as can be seen, be reduced according to the tantalum of the inventive method refining preparation and/or O, C, N, H, the impurity atom content such as K, Na of niobium powder, specific surface area reduces, and loose density increases.This tantalum and/or niobium powder are suitable as the raw material of powder used in metallurgy.
Claims (5)
1. powder used in metallurgy tantalum and/or niobium powder, the oxygen level of tantalum powder and/or niobium powder is not higher than 1500ppm, and nitrogen content is not higher than 200ppm, and the specific surface area of tantalum powder is not more than 0.15m
2/ g, loose density is at 3.5～7.0g/cm
3In the scope, niobium powder specific surface area is not more than 0.30m
2/ g, loose density is at 2.0～4.0g/cm
3In the scope.
2. the preparation method of powder used in metallurgy tantalum as claimed in claim 1 and/or niobium powder, its production stage comprises: (1) is pressed into the base bar to raw material tantalum and/or niobium powder raw material; (2) the base bar of vacuum sintering compacting; (3) with sintered blank bar hydrogenation powder process; (4) hydrogenant tantalum and/or niobium powder adding reducing metal are carried out deoxidation, dehydrogenation thermal treatment; (5) tantalum after the thermal treatment and/or niobium powder are carried out pickling, washing, oven dry.
3. powder used in metallurgy tantalum as claimed in claim 1 and/or niobium powder is characterized in that it is serves as the main powder that contains micro-grain-refining agent element with the tantalum powder.
4. powder used in metallurgy tantalum as claimed in claim 1 and/or niobium powder is characterized in that it is serves as the main powder that contains micro-grain-refining agent element with the niobium powder.
5. as claim 3 or 4 described powder used in metallurgy tantalum and/or niobium powders, it is characterized in that described micro-grain-refining agent element is silicon and/or yttrium.
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